# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_200k
_database_code_depnum_ccdc_archive 'CCDC 1493439'
_audit_update_record             
;
2016-07-14 deposited with the CCDC.
2016-12-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H24 Fe N24, 2(C F3 O3 S)'
_chemical_formula_sum            'C14 H24 F6 Fe N24 O6 S2'
_chemical_formula_weight         858.54

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0040 0.0020
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
H H 0.0000 0.0000
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
N N 0.0076 0.0040
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
O O 0.0132 0.0074
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
F F 0.0211 0.0125
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
S S 0.1431 0.1480
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
Fe Fe 0.3555 0.9930
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.5430(10)
_cell_length_b                   11.336(2)
_cell_length_c                   11.424(2)
_cell_angle_alpha                63.483(3)
_cell_angle_beta                 89.755(4)
_cell_angle_gamma                88.763(4)
_cell_volume                     873.9(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    7352
_cell_measurement_theta_min      3.63
_cell_measurement_theta_max      33.66

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.631
_exptl_crystal_F_000             436
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    0.820
_shelx_estimated_absorpt_T_min   0.922
_shelx_estimated_absorpt_T_max   0.968
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.656
_exptl_absorpt_correction_T_max  0.747
_exptl_absorpt_process_details   'SADABS-2014/5 - Bruker AXS'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.7749
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'Advanced Light Source station 11.3.1'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'Bruker D8 with PHOTON 100 detector'
_diffrn_measurement_method       'shutterless /f and /w scans'
_diffrn_detector_area_resol_mean 10.42
_diffrn_reflns_number            14797
_diffrn_reflns_av_unetI/netI     0.0393
_diffrn_reflns_av_R_equivalents  0.0341
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.172
_diffrn_reflns_theta_max         33.072
_diffrn_reflns_theta_full        33.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             5098
_reflns_number_gt                4107
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX 2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2015)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 All non-hydrogens were refined anisotropically. The triflate ion
 is disordered over two inverted positions with relative occupancies
 0.769:0.231 and was refined with displacement parameters restraints.
 Hydrogens were found in a difference Fourier map, placed geometrically
 on their carrier atom and refined with a riding model.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0709P)²+0.5176P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5098
_refine_ls_number_parameters     317
_refine_ls_number_restraints     272
_refine_ls_R_factor_all          0.0652
_refine_ls_R_factor_gt           0.0509
_refine_ls_wR_factor_ref         0.1457
_refine_ls_wR_factor_gt          0.1353
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_restrained_S_all      1.181
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.5000 0.5000 0.5000 0.02819(12) Uani 1 2 d S . P . .
N1 N 0.6672(2) 0.67138(17) 0.43034(17) 0.0342(4) Uani 1 1 d . . . . .
N2 N 0.7643(3) 0.7126(2) 0.3193(2) 0.0511(5) Uani 1 1 d . . . . .
N3 N 0.8385(3) 0.8226(2) 0.2946(2) 0.0538(6) Uani 1 1 d . . . . .
N4 N 0.7905(2) 0.85391(18) 0.39075(18) 0.0350(4) Uani 1 1 d . . . . .
N5 N 0.6749(2) 0.40809(17) 0.40823(18) 0.0350(4) Uani 1 1 d . . . . .
N6 N 0.7520(4) 0.2877(2) 0.4772(2) 0.0548(6) Uani 1 1 d . . . . .
N7 N 0.8537(3) 0.2588(2) 0.4022(2) 0.0527(6) Uani 1 1 d . . . . .
N8 N 0.8437(3) 0.35996(18) 0.2838(2) 0.0383(4) Uani 1 1 d . . . . .
N9 N 0.6570(3) 0.40164(18) 0.67954(17) 0.0361(4) Uani 1 1 d . . . . .
N10 N 0.7557(3) 0.4649(2) 0.7310(2) 0.0557(6) Uani 1 1 d . . . . .
N11 N 0.8441(3) 0.3787(3) 0.8315(2) 0.0636(7) Uani 1 1 d . . . . .
N12 N 0.8017(3) 0.2604(2) 0.8461(2) 0.0486(5) Uani 1 1 d . . . . .
C1 C 0.6864(3) 0.7614(2) 0.4724(2) 0.0346(4) Uani 1 1 d . . . . .
H1A H 0.6340 0.7599 0.5488 0.041 Uiso 1 1 calc R U . . .
C2 C 0.8413(4) 0.9780(3) 0.3901(3) 0.0498(6) Uani 1 1 d . . . . .
H2A H 0.9671 0.9931 0.3679 0.075 Uiso 1 1 calc R U . . .
H2B H 0.8212 0.9732 0.4769 0.075 Uiso 1 1 calc R U . . .
H2C H 0.7697 1.0507 0.3251 0.075 Uiso 1 1 calc R U . . .
C3 C 0.7344(4) 0.4500(2) 0.2893(2) 0.0457(6) Uani 1 1 d . . . . .
H3A H 0.7040 0.5324 0.2178 0.055 Uiso 1 1 calc R U . . .
C4 C 0.9459(5) 0.3598(3) 0.1748(3) 0.0648(8) Uani 1 1 d . . . . .
H4A H 1.0092 0.2749 0.2036 0.097 Uiso 1 1 calc R U . . .
H4B H 1.0315 0.4310 0.1452 0.097 Uiso 1 1 calc R U . . .
H4C H 0.8653 0.3732 0.1026 0.097 Uiso 1 1 calc R U . . .
C5 C 0.6878(4) 0.2741(2) 0.7533(2) 0.0465(6) Uani 1 1 d . . . . .
H5A H 0.6366 0.2043 0.7415 0.056 Uiso 1 1 calc R U . . .
C6 C 0.8743(6) 0.1387(4) 0.9526(3) 0.0812(12) Uani 1 1 d . . . . .
H6A H 0.9901 0.1561 0.9796 0.122 Uiso 1 1 calc R U . . .
H6B H 0.8881 0.0708 0.9221 0.122 Uiso 1 1 calc R U . . .
H6C H 0.7932 0.1080 1.0271 0.122 Uiso 1 1 calc R U . . .
S1 S 0.36477(12) 0.10525(8) 0.21478(8) 0.0460(3) Uani 0.770(2) 1 d . U P A 1
O1 O 0.4880(7) 0.0090(5) 0.2066(4) 0.0626(11) Uani 0.770(2) 1 d . U P A 1
O2 O 0.1828(6) 0.0897(5) 0.1932(7) 0.0958(15) Uani 0.770(2) 1 d . U P A 1
O3 O 0.3854(8) 0.1403(5) 0.3156(4) 0.1139(14) Uani 0.770(2) 1 d . U P A 1
C7 C 0.4167(8) 0.2522(5) 0.0682(6) 0.0760(10) Uani 0.770(2) 1 d . U P A 1
F1 F 0.3220(6) 0.3553(3) 0.0533(5) 0.1151(16) Uani 0.770(2) 1 d . U P A 1
F2 F 0.5856(6) 0.2836(5) 0.0677(5) 0.1232(14) Uani 0.770(2) 1 d . U P A 1
F3 F 0.4130(6) 0.2405(5) -0.0358(3) 0.1368(13) Uani 0.770(2) 1 d . U P A 1
S2 S 0.4192(5) 0.2485(4) 0.1279(4) 0.0505(8) Uani 0.230(2) 1 d . U P A 2
O4 O 0.399(2) 0.2323(15) 0.2563(12) 0.089(3) Uani 0.230(2) 1 d . U P A 2
O5 O 0.2655(19) 0.3178(16) 0.0248(13) 0.082(3) Uani 0.230(2) 1 d . U P A 2
O6 O 0.601(2) 0.2544(19) 0.1259(14) 0.083(3) Uani 0.230(2) 1 d . U P A 2
C8 C 0.373(2) 0.0892(15) 0.1318(15) 0.0635(15) Uani 0.230(2) 1 d . U P A 2
F4 F 0.3825(17) 0.1017(14) 0.0139(11) 0.105(3) Uani 0.230(2) 1 d . U P A 2
F5 F 0.454(2) -0.0068(16) 0.2494(14) 0.074(3) Uani 0.230(2) 1 d . U P A 2
F6 F 0.2031(18) 0.0530(16) 0.1726(16) 0.086(3) Uani 0.230(2) 1 d . U P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N1 2.1712(18) 2_666 ?
Fe1 N1 2.1712(18) . ?
Fe1 N9 2.1852(18) . ?
Fe1 N9 2.1852(18) 2_666 ?
Fe1 N5 2.1975(17) 2_666 ?
Fe1 N5 2.1975(17) . ?
N1 C1 1.318(3) . ?
N1 N2 1.357(3) . ?
N2 N3 1.290(3) . ?
N3 N4 1.342(3) . ?
N4 C1 1.320(3) . ?
N4 C2 1.462(3) . ?
N5 C3 1.305(3) . ?
N5 N6 1.354(3) . ?
N6 N7 1.290(3) . ?
N7 N8 1.327(3) . ?
N8 C3 1.321(3) . ?
N8 C4 1.462(3) . ?
N9 C5 1.325(3) . ?
N9 N10 1.348(3) . ?
N10 N11 1.301(3) . ?
N11 N12 1.321(4) . ?
N12 C5 1.319(3) . ?
N12 C6 1.469(3) . ?
C1 H1A 0.9500 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9500 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9500 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
S1 O3 1.387(3) . ?
S1 O2 1.424(5) . ?
S1 O1 1.453(5) . ?
S1 C7 1.806(5) . ?
C7 F3 1.253(8) . ?
C7 F1 1.301(7) . ?
C7 F2 1.329(8) . ?
S2 O6 1.372(16) . ?
S2 O4 1.403(11) . ?
S2 O5 1.579(13) . ?
S2 C8 1.828(15) . ?
C8 F4 1.292(17) . ?
C8 F6 1.37(2) . ?
C8 F5 1.43(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Fe1 N1 180.0 2_666 . ?
N1 Fe1 N9 88.75(7) 2_666 . ?
N1 Fe1 N9 91.25(7) . . ?
N1 Fe1 N9 91.25(7) 2_666 2_666 ?
N1 Fe1 N9 88.75(7) . 2_666 ?
N9 Fe1 N9 180.00(8) . 2_666 ?
N1 Fe1 N5 90.59(7) 2_666 2_666 ?
N1 Fe1 N5 89.41(7) . 2_666 ?
N9 Fe1 N5 91.07(7) . 2_666 ?
N9 Fe1 N5 88.93(7) 2_666 2_666 ?
N1 Fe1 N5 89.41(7) 2_666 . ?
N1 Fe1 N5 90.59(7) . . ?
N9 Fe1 N5 88.93(7) . . ?
N9 Fe1 N5 91.07(7) 2_666 . ?
N5 Fe1 N5 180.0 2_666 . ?
C1 N1 N2 105.77(18) . . ?
C1 N1 Fe1 130.89(15) . . ?
N2 N1 Fe1 123.06(14) . . ?
N3 N2 N1 110.24(19) . . ?
N2 N3 N4 106.62(19) . . ?
C1 N4 N3 108.64(18) . . ?
C1 N4 C2 129.4(2) . . ?
N3 N4 C2 121.8(2) . . ?
C3 N5 N6 105.50(18) . . ?
C3 N5 Fe1 132.20(15) . . ?
N6 N5 Fe1 122.23(14) . . ?
N7 N6 N5 110.1(2) . . ?
N6 N7 N8 106.96(19) . . ?
C3 N8 N7 108.19(19) . . ?
C3 N8 C4 130.7(2) . . ?
N7 N8 C4 121.1(2) . . ?
C5 N9 N10 106.1(2) . . ?
C5 N9 Fe1 129.38(17) . . ?
N10 N9 Fe1 124.35(14) . . ?
N11 N10 N9 109.4(2) . . ?
N10 N11 N12 107.4(2) . . ?
C5 N12 N11 108.8(2) . . ?
C5 N12 C6 128.8(3) . . ?
N11 N12 C6 122.4(3) . . ?
N1 C1 N4 108.72(19) . . ?
N1 C1 H1A 125.6 . . ?
N4 C1 H1A 125.6 . . ?
N4 C2 H2A 109.5 . . ?
N4 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
N4 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N5 C3 N8 109.3(2) . . ?
N5 C3 H3A 125.4 . . ?
N8 C3 H3A 125.4 . . ?
N8 C4 H4A 109.5 . . ?
N8 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N8 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N12 C5 N9 108.4(2) . . ?
N12 C5 H5A 125.8 . . ?
N9 C5 H5A 125.8 . . ?
N12 C6 H6A 109.5 . . ?
N12 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
N12 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
O3 S1 O2 111.5(4) . . ?
O3 S1 O1 118.7(3) . . ?
O2 S1 O1 115.9(3) . . ?
O3 S1 C7 104.7(3) . . ?
O2 S1 C7 101.5(3) . . ?
O1 S1 C7 101.7(3) . . ?
F3 C7 F1 109.2(6) . . ?
F3 C7 F2 99.5(5) . . ?
F1 C7 F2 106.7(6) . . ?
F3 C7 S1 115.4(5) . . ?
F1 C7 S1 113.6(4) . . ?
F2 C7 S1 111.3(4) . . ?
O6 S2 O4 96.2(10) . . ?
O6 S2 O5 135.2(8) . . ?
O4 S2 O5 119.4(9) . . ?
O6 S2 C8 104.7(11) . . ?
O4 S2 C8 106.6(8) . . ?
O5 S2 C8 91.2(8) . . ?
F4 C8 F6 106.5(13) . . ?
F4 C8 F5 129.9(15) . . ?
F6 C8 F5 94.9(13) . . ?
F4 C8 S2 108.4(11) . . ?
F6 C8 S2 110.6(12) . . ?
F5 C8 S2 105.3(11) . . ?

_refine_diff_density_max         0.825
_refine_diff_density_min         -0.663
_refine_diff_density_rms         0.068

_shelxl_version_number           2014-3


_exptl_crystal_preparation       ', Magnetic properties'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_85K
_database_code_depnum_ccdc_archive 'CCDC 1493440'
_audit_update_record             
;
2016-07-14 deposited with the CCDC.
2016-12-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H24 Fe N24, 2(C F3 O3 S)'
_chemical_formula_sum            'C14 H24 F6 Fe N24 O6 S2'
_chemical_formula_weight         858.54

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0040 0.0020
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
H H 0.0000 0.0000
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
N N 0.0076 0.0040
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
O O 0.0132 0.0074
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
F F 0.0211 0.0125
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
S S 0.1431 0.1480
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
Fe Fe 0.3555 0.9930
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'

_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3 :H'
_space_group_name_Hall           '-R 3'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   19.724(4)
_cell_length_b                   19.724(4)
_cell_length_c                   45.031(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     15172(7)
_cell_formula_units_Z            18
_cell_measurement_temperature    84(2)
_cell_measurement_reflns_used    7055
_cell_measurement_theta_min      3.25
_cell_measurement_theta_max      26.00

_exptl_crystal_description       block
_exptl_crystal_colour            'light purple'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.691
_exptl_crystal_F_000             7848
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    0.850
_shelx_estimated_absorpt_T_min   0.905
_shelx_estimated_absorpt_T_max   0.951
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.668
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_process_details   'SADABS-2008/1 - Bruker AXS'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      85(2)
_diffrn_radiation_wavelength     0.7749
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'Advanced Light Source station 11.3.1'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'Bruker APEX II CCD diffractometer'
_diffrn_measurement_method       'ω rotation with narrow frames'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            28853
_diffrn_reflns_av_unetI/netI     0.0490
_diffrn_reflns_av_R_equivalents  0.0821
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_theta_min         3.264
_diffrn_reflns_theta_max         26.077
_diffrn_reflns_theta_full        26.120
_diffrn_measured_fraction_theta_max 0.842
_diffrn_measured_fraction_theta_full 0.839
_diffrn_reflns_Laue_measured_fraction_max 0.842
_diffrn_reflns_Laue_measured_fraction_full 0.839
_diffrn_reflns_point_group_measured_fraction_max 0.842
_diffrn_reflns_point_group_measured_fraction_full 0.839
_reflns_number_total             4360
_reflns_number_gt                3400
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX 2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2015)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 All non-hydrogens were refined anisotropically. Hydrogens were
 found in a difference Fourier map, placed geometrically on their
 carrier atom and refined with a riding model.
;

_vrf_THETM01_85K                 
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575
            Calculated sin(theta_max)/wavelength =    0.5673
RESPONSE: The compound suffers several structural transitions that
affect the quality of the diffraction. This dataset corresponds to
a crystal that has first been mounted at 200 K, thus passing rapidly
the order-disorder transition occurring at ca. 300 K, and then been
cooled down slowly from 200 K. The present rather poor diffraction is
likely due to crystal damage upon passing additional transitions at ca.
190 and 160 K. The results are low values of thetamax and thetafull, as
well as non-ideal data/parameter ratio.
;

_vrf_REFNR01_85K                 
;
PROBLEM: Ratio of reflections to parameters is < 10 for a
            centrosymmetric structure
            sine(theta)/lambda                0.5673
            Proportion of unique data used    1.0000
            Ratio reflections to parameters   9.0083
RESPONSE: The compound suffers several structural transitions that
affect the quality of the diffraction. This dataset corresponds to
a crystal that has first been mounted at 200 K, thus passing rapidly
the order-disorder transition occurring at ca. 300 K, and then been
cooled down slowly from 200 K. The present rather poor diffraction is
likely due to crystal damage upon passing additional transitions at ca.
190 and 160 K. The results are low values of thetamax and thetafull, as
well as non-ideal data/parameter ratio.
;

_vrf_PLAT088_85K                 
;
PROBLEM: Poor Data / Parameter Ratio ....................       9.01 Note
RESPONSE: The compound suffers several structural transitions that
affect the quality of the diffraction. This dataset corresponds to
a crystal that has first been mounted at 200 K, thus passing rapidly
the order-disorder transition occurring at ca. 300 K, and then been
cooled down slowly from 200 K. The present rather poor diffraction is
likely due to crystal damage upon passing additional transitions at ca.
190 and 160 K. The results are low values of thetamax and thetafull, as
well as non-ideal data/parameter ratio.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0416P)²+42.8581P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4360
_refine_ls_number_parameters     484
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0609
_refine_ls_R_factor_gt           0.0403
_refine_ls_wR_factor_ref         0.1087
_refine_ls_wR_factor_gt          0.0940
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_restrained_S_all      1.082
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.3333 0.6667 0.58664(2) 0.0178(2) Uani 1 3 d S T P . .
Fe2 Fe 0.0000 0.0000 0.58800(2) 0.0190(2) Uani 1 3 d S T P . .
Fe3 Fe 0.6667 0.3333 0.58258(2) 0.0184(2) Uani 1 3 d S T P . .
N1 N 0.42213(16) 0.68062(16) 0.61174(6) 0.0202(6) Uani 1 1 d . . . . .
N2 N 0.42037(18) 0.62141(17) 0.62827(7) 0.0266(7) Uani 1 1 d . . . . .
N3 N 0.48654(18) 0.64671(18) 0.64187(7) 0.0265(7) Uani 1 1 d . . . . .
N4 N 0.53176(16) 0.72264(16) 0.63432(6) 0.0207(6) Uani 1 1 d . . . . .
N5 N 0.34968(16) 0.59358(16) 0.56144(6) 0.0206(6) Uani 1 1 d . . . . .
N6 N 0.29695(18) 0.54388(18) 0.54095(6) 0.0277(7) Uani 1 1 d . . . . .
N7 N 0.32440(19) 0.5042(2) 0.52799(7) 0.0303(7) Uani 1 1 d . . . . .
N8 N 0.39563(17) 0.52790(17) 0.53969(6) 0.0233(7) Uani 1 1 d . . . . .
N9 N 0.09052(17) 0.08976(17) 0.55995(6) 0.0228(7) Uani 1 1 d . . . . .
N10 N 0.14693(18) 0.07990(18) 0.54648(7) 0.0282(7) Uani 1 1 d . . . . .
N11 N 0.19165(18) 0.14090(19) 0.53035(7) 0.0292(7) Uani 1 1 d . . . . .
N12 N 0.16374(17) 0.19051(17) 0.53321(6) 0.0220(6) Uani 1 1 d . . . . .
N13 N 0.08678(17) -0.00584(17) 0.61629(6) 0.0234(7) Uani 1 1 d . . . . .
N14 N 0.07211(19) -0.07061(19) 0.63213(7) 0.0307(7) Uani 1 1 d . . . . .
N15 N 0.13257(18) -0.05531(18) 0.64802(7) 0.0306(7) Uani 1 1 d . . . . .
N16 N 0.18706(17) 0.01921(17) 0.64284(6) 0.0218(6) Uani 1 1 d . . . . .
N17 N 0.66665(17) 0.24349(17) 0.55286(6) 0.0221(6) Uani 1 1 d . . . . .
N18 N 0.59819(18) 0.17882(17) 0.54468(7) 0.0263(7) Uani 1 1 d . . . . .
N19 N 0.61205(18) 0.13765(18) 0.52600(6) 0.0266(7) Uani 1 1 d . . . . .
N20 N 0.69046(17) 0.17552(17) 0.52164(6) 0.0236(7) Uani 1 1 d . . . . .
N21 N 0.57791(17) 0.24023(17) 0.60939(6) 0.0217(6) Uani 1 1 d . . . . .
N22 N 0.51923(18) 0.24696(18) 0.62277(7) 0.0286(7) Uani 1 1 d . . . . .
N23 N 0.47004(18) 0.18138(18) 0.63509(7) 0.0283(7) Uani 1 1 d . . . . .
N24 N 0.49662(17) 0.13137(17) 0.62996(6) 0.0216(6) Uani 1 1 d . . . . .
C1 C 0.4919(2) 0.7424(2) 0.61580(7) 0.0211(7) Uani 1 1 d . . . . .
H1A H 0.5105 0.7924 0.6070 0.025 Uiso 1 1 calc R U . . .
C2 C 0.6118(2) 0.7701(2) 0.64500(8) 0.0262(8) Uani 1 1 d . . . . .
H2A H 0.6264 0.8254 0.6448 0.039 Uiso 1 1 calc R U . . .
H2B H 0.6473 0.7624 0.6321 0.039 Uiso 1 1 calc R U . . .
H2C H 0.6155 0.7544 0.6653 0.039 Uiso 1 1 calc R U . . .
C3 C 0.4103(2) 0.5822(2) 0.56014(7) 0.0228(8) Uani 1 1 d . . . . .
H3A H 0.4564 0.6084 0.5718 0.027 Uiso 1 1 calc R U . . .
C4 C 0.4409(2) 0.4905(2) 0.53187(8) 0.0285(8) Uani 1 1 d . . . . .
H4A H 0.4962 0.5258 0.5366 0.043 Uiso 1 1 calc R U . . .
H4B H 0.4354 0.4786 0.5106 0.043 Uiso 1 1 calc R U . . .
H4C H 0.4216 0.4418 0.5432 0.043 Uiso 1 1 calc R U . . .
C5 C 0.1023(2) 0.1588(2) 0.55146(7) 0.0216(7) Uani 1 1 d . . . . .
H5A H 0.0722 0.1819 0.5573 0.026 Uiso 1 1 calc R U . . .
C6 C 0.2021(2) 0.2670(2) 0.51866(8) 0.0293(8) Uani 1 1 d . . . . .
H6A H 0.1625 0.2759 0.5091 0.044 Uiso 1 1 calc R U . . .
H6B H 0.2387 0.2685 0.5036 0.044 Uiso 1 1 calc R U . . .
H6C H 0.2308 0.3080 0.5335 0.044 Uiso 1 1 calc R U . . .
C7 C 0.1582(2) 0.0480(2) 0.62336(8) 0.0242(8) Uani 1 1 d . . . . .
H7A H 0.1849 0.0998 0.6157 0.029 Uiso 1 1 calc R U . . .
C8 C 0.2641(2) 0.0553(2) 0.65666(8) 0.0290(8) Uani 1 1 d . . . . .
H8A H 0.3045 0.0823 0.6415 0.044 Uiso 1 1 calc R U . . .
H8B H 0.2716 0.0147 0.6661 0.044 Uiso 1 1 calc R U . . .
H8C H 0.2681 0.0930 0.6717 0.044 Uiso 1 1 calc R U . . .
C9 C 0.7218(2) 0.2395(2) 0.53803(7) 0.0251(8) Uani 1 1 d . . . . .
H9A H 0.7761 0.2769 0.5390 0.030 Uiso 1 1 calc R U . . .
C10 C 0.7255(2) 0.1439(2) 0.50116(8) 0.0328(9) Uani 1 1 d . . . . .
H10A H 0.7826 0.1766 0.5018 0.049 Uiso 1 1 calc R U . . .
H10B H 0.7070 0.1437 0.4809 0.049 Uiso 1 1 calc R U . . .
H10C H 0.7102 0.0903 0.5070 0.049 Uiso 1 1 calc R U . . .
C11 C 0.5621(2) 0.1679(2) 0.61437(7) 0.0217(8) Uani 1 1 d . . . . .
H11A H 0.5926 0.1458 0.6079 0.026 Uiso 1 1 calc R U . . .
C12 C 0.4520(2) 0.0495(2) 0.63950(8) 0.0271(8) Uani 1 1 d . . . . .
H12A H 0.4827 0.0238 0.6357 0.041 Uiso 1 1 calc R U . . .
H12B H 0.4027 0.0226 0.6284 0.041 Uiso 1 1 calc R U . . .
H12C H 0.4406 0.0473 0.6608 0.041 Uiso 1 1 calc R U . . .
S1 S 0.35378(5) 0.37521(5) 0.60513(2) 0.0231(2) Uani 1 1 d . . . . .
O1 O 0.31660(15) 0.40330(15) 0.58487(5) 0.0292(6) Uani 1 1 d . . . . .
O2 O 0.32422(15) 0.36201(15) 0.63503(5) 0.0310(6) Uani 1 1 d . . . . .
O3 O 0.43757(15) 0.41284(16) 0.60247(6) 0.0370(7) Uani 1 1 d . . . . .
C13 C 0.3218(2) 0.2772(2) 0.59154(8) 0.0278(8) Uani 1 1 d . . . . .
F1 F 0.24387(13) 0.23204(13) 0.59244(5) 0.0411(6) Uani 1 1 d . . . . .
F2 F 0.34388(14) 0.27818(14) 0.56323(5) 0.0376(6) Uani 1 1 d . . . . .
F3 F 0.35076(16) 0.24027(14) 0.60739(5) 0.0473(7) Uani 1 1 d . . . . .
S2 S 0.28913(5) -0.03311(5) 0.56756(2) 0.0242(2) Uani 1 1 d . . . . .
O4 O 0.23236(14) -0.05981(15) 0.54403(5) 0.0299(6) Uani 1 1 d . . . . .
O5 O 0.33390(17) -0.07225(17) 0.57000(6) 0.0374(7) Uani 1 1 d . . . . .
O6 O 0.26356(17) -0.01774(16) 0.59533(5) 0.0367(7) Uani 1 1 d . . . . .
C14 C 0.3612(2) 0.0644(2) 0.55524(8) 0.0327(9) Uani 1 1 d . . . . .
F4 F 0.33106(15) 0.11126(13) 0.55175(5) 0.0430(6) Uani 1 1 d . . . . .
F5 F 0.39232(14) 0.06225(16) 0.52879(5) 0.0472(7) Uani 1 1 d . . . . .
F6 F 0.42087(15) 0.09969(15) 0.57410(5) 0.0529(7) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N5 1.984(3) 3_565 ?
Fe1 N5 1.983(3) 2_665 ?
Fe1 N5 1.983(3) . ?
Fe1 N1 1.985(3) 2_665 ?
Fe1 N1 1.985(3) 3_565 ?
Fe1 N1 1.985(3) . ?
Fe2 N9 2.181(3) 3 ?
Fe2 N9 2.181(3) 2 ?
Fe2 N9 2.181(3) . ?
Fe2 N13 2.183(3) 3 ?
Fe2 N13 2.183(3) 2 ?
Fe2 N13 2.183(3) . ?
Fe3 N21 2.163(3) . ?
Fe3 N21 2.163(3) 2_655 ?
Fe3 N21 2.163(3) 3_665 ?
Fe3 N17 2.221(3) . ?
Fe3 N17 2.221(3) 2_655 ?
Fe3 N17 2.221(3) 3_665 ?
N1 C1 1.317(5) . ?
N1 N2 1.370(4) . ?
N2 N3 1.295(4) . ?
N3 N4 1.349(4) . ?
N4 C1 1.331(4) . ?
N4 C2 1.457(5) . ?
N5 C3 1.323(5) . ?
N5 N6 1.369(4) . ?
N6 N7 1.293(4) . ?
N7 N8 1.347(4) . ?
N8 C3 1.330(4) . ?
N8 C4 1.459(5) . ?
N9 C5 1.318(5) . ?
N9 N10 1.364(4) . ?
N10 N11 1.301(4) . ?
N11 N12 1.347(4) . ?
N12 C5 1.333(5) . ?
N12 C6 1.462(4) . ?
N13 C7 1.310(5) . ?
N13 N14 1.362(4) . ?
N14 N15 1.291(4) . ?
N15 N16 1.338(4) . ?
N16 C7 1.320(5) . ?
N16 C8 1.457(5) . ?
N17 C9 1.313(5) . ?
N17 N18 1.365(4) . ?
N18 N19 1.290(4) . ?
N19 N20 1.354(4) . ?
N20 C9 1.319(5) . ?
N20 C10 1.465(5) . ?
N21 C11 1.318(5) . ?
N21 N22 1.369(4) . ?
N22 N23 1.291(4) . ?
N23 N24 1.349(4) . ?
N24 C11 1.323(5) . ?
N24 C12 1.465(5) . ?
C1 H1A 0.9500 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9500 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9500 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9500 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9500 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9500 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
S1 O2 1.438(3) . ?
S1 O3 1.439(3) . ?
S1 O1 1.443(3) . ?
S1 C13 1.814(4) . ?
C13 F3 1.334(4) . ?
C13 F1 1.338(5) . ?
C13 F2 1.344(4) . ?
S2 O6 1.436(3) . ?
S2 O4 1.437(3) . ?
S2 O5 1.439(3) . ?
S2 C14 1.814(4) . ?
C14 F6 1.331(4) . ?
C14 F4 1.336(5) . ?
C14 F5 1.350(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N5 Fe1 N5 90.53(11) 3_565 2_665 ?
N5 Fe1 N5 90.53(11) 3_565 . ?
N5 Fe1 N5 90.53(11) 2_665 . ?
N5 Fe1 N1 90.23(11) 3_565 2_665 ?
N5 Fe1 N1 88.49(11) 2_665 2_665 ?
N5 Fe1 N1 178.77(11) . 2_665 ?
N5 Fe1 N1 88.49(11) 3_565 3_565 ?
N5 Fe1 N1 178.77(11) 2_665 3_565 ?
N5 Fe1 N1 90.23(11) . 3_565 ?
N1 Fe1 N1 90.76(11) 2_665 3_565 ?
N5 Fe1 N1 178.77(11) 3_565 . ?
N5 Fe1 N1 90.23(11) 2_665 . ?
N5 Fe1 N1 88.49(11) . . ?
N1 Fe1 N1 90.76(11) 2_665 . ?
N1 Fe1 N1 90.76(11) 3_565 . ?
N9 Fe2 N9 89.82(11) 3 2 ?
N9 Fe2 N9 89.82(11) 3 . ?
N9 Fe2 N9 89.82(11) 2 . ?
N9 Fe2 N13 92.04(11) 3 3 ?
N9 Fe2 N13 88.83(11) 2 3 ?
N9 Fe2 N13 177.69(10) . 3 ?
N9 Fe2 N13 177.70(10) 3 2 ?
N9 Fe2 N13 92.04(11) 2 2 ?
N9 Fe2 N13 88.83(11) . 2 ?
N13 Fe2 N13 89.35(11) 3 2 ?
N9 Fe2 N13 88.83(11) 3 . ?
N9 Fe2 N13 177.70(10) 2 . ?
N9 Fe2 N13 92.04(11) . . ?
N13 Fe2 N13 89.36(11) 3 . ?
N13 Fe2 N13 89.36(11) 2 . ?
N21 Fe3 N21 91.89(11) . 2_655 ?
N21 Fe3 N21 91.89(11) . 3_665 ?
N21 Fe3 N21 91.89(11) 2_655 3_665 ?
N21 Fe3 N17 88.95(11) . . ?
N21 Fe3 N17 91.68(10) 2_655 . ?
N21 Fe3 N17 176.31(11) 3_665 . ?
N21 Fe3 N17 176.30(11) . 2_655 ?
N21 Fe3 N17 88.96(11) 2_655 2_655 ?
N21 Fe3 N17 91.68(11) 3_665 2_655 ?
N17 Fe3 N17 87.42(11) . 2_655 ?
N21 Fe3 N17 91.69(11) . 3_665 ?
N21 Fe3 N17 176.30(11) 2_655 3_665 ?
N21 Fe3 N17 88.96(11) 3_665 3_665 ?
N17 Fe3 N17 87.42(11) . 3_665 ?
N17 Fe3 N17 87.42(11) 2_655 3_665 ?
C1 N1 N2 106.4(3) . . ?
C1 N1 Fe1 130.4(2) . . ?
N2 N1 Fe1 123.1(2) . . ?
N3 N2 N1 109.7(3) . . ?
N2 N3 N4 106.7(3) . . ?
C1 N4 N3 108.9(3) . . ?
C1 N4 C2 128.9(3) . . ?
N3 N4 C2 122.2(3) . . ?
C3 N5 N6 106.0(3) . . ?
C3 N5 Fe1 129.6(2) . . ?
N6 N5 Fe1 124.4(2) . . ?
N7 N6 N5 109.9(3) . . ?
N6 N7 N8 107.0(3) . . ?
C3 N8 N7 108.6(3) . . ?
C3 N8 C4 129.3(3) . . ?
N7 N8 C4 121.8(3) . . ?
C5 N9 N10 106.5(3) . . ?
C5 N9 Fe2 131.0(2) . . ?
N10 N9 Fe2 122.5(2) . . ?
N11 N10 N9 109.9(3) . . ?
N10 N11 N12 106.5(3) . . ?
C5 N12 N11 108.9(3) . . ?
C5 N12 C6 129.8(3) . . ?
N11 N12 C6 121.2(3) . . ?
C7 N13 N14 105.8(3) . . ?
C7 N13 Fe2 130.7(2) . . ?
N14 N13 Fe2 123.4(2) . . ?
N15 N14 N13 109.4(3) . . ?
N14 N15 N16 107.5(3) . . ?
C7 N16 N15 107.8(3) . . ?
C7 N16 C8 130.0(3) . . ?
N15 N16 C8 122.1(3) . . ?
C9 N17 N18 105.6(3) . . ?
C9 N17 Fe3 133.3(2) . . ?
N18 N17 Fe3 120.9(2) . . ?
N19 N18 N17 110.0(3) . . ?
N18 N19 N20 106.9(3) . . ?
C9 N20 N19 107.9(3) . . ?
C9 N20 C10 131.6(3) . . ?
N19 N20 C10 120.5(3) . . ?
C11 N21 N22 106.0(3) . . ?
C11 N21 Fe3 131.8(2) . . ?
N22 N21 Fe3 121.9(2) . . ?
N23 N22 N21 109.9(3) . . ?
N22 N23 N24 106.7(3) . . ?
C11 N24 N23 108.9(3) . . ?
C11 N24 C12 129.9(3) . . ?
N23 N24 C12 121.1(3) . . ?
N1 C1 N4 108.2(3) . . ?
N1 C1 H1A 125.9 . . ?
N4 C1 H1A 125.9 . . ?
N4 C2 H2A 109.5 . . ?
N4 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
N4 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N5 C3 N8 108.4(3) . . ?
N5 C3 H3A 125.8 . . ?
N8 C3 H3A 125.8 . . ?
N8 C4 H4A 109.5 . . ?
N8 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N8 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N9 C5 N12 108.2(3) . . ?
N9 C5 H5A 125.9 . . ?
N12 C5 H5A 125.9 . . ?
N12 C6 H6A 109.5 . . ?
N12 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
N12 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N13 C7 N16 109.4(3) . . ?
N13 C7 H7A 125.3 . . ?
N16 C7 H7A 125.3 . . ?
N16 C8 H8A 109.5 . . ?
N16 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N16 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N17 C9 N20 109.6(3) . . ?
N17 C9 H9A 125.2 . . ?
N20 C9 H9A 125.2 . . ?
N20 C10 H10A 109.5 . . ?
N20 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
N20 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N21 C11 N24 108.6(3) . . ?
N21 C11 H11A 125.7 . . ?
N24 C11 H11A 125.7 . . ?
N24 C12 H12A 109.5 . . ?
N24 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N24 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O2 S1 O3 115.37(16) . . ?
O2 S1 O1 115.05(16) . . ?
O3 S1 O1 114.98(16) . . ?
O2 S1 C13 103.27(16) . . ?
O3 S1 C13 102.64(17) . . ?
O1 S1 C13 102.92(16) . . ?
F3 C13 F1 106.5(3) . . ?
F3 C13 F2 107.0(3) . . ?
F1 C13 F2 107.1(3) . . ?
F3 C13 S1 112.7(2) . . ?
F1 C13 S1 111.7(3) . . ?
F2 C13 S1 111.5(3) . . ?
O6 S2 O4 115.34(17) . . ?
O6 S2 O5 114.93(17) . . ?
O4 S2 O5 115.75(16) . . ?
O6 S2 C14 102.39(18) . . ?
O4 S2 C14 102.54(16) . . ?
O5 S2 C14 103.04(19) . . ?
F6 C14 F4 107.2(3) . . ?
F6 C14 F5 106.5(3) . . ?
F4 C14 F5 106.5(3) . . ?
F6 C14 S2 112.3(3) . . ?
F4 C14 S2 112.6(3) . . ?
F5 C14 S2 111.4(3) . . ?

_refine_diff_density_max         0.245
_refine_diff_density_min         -0.325
_refine_diff_density_rms         0.061

_shelxl_version_number           2014-3


_exptl_crystal_preparation       ', Magnetic properties'
